JPS6348806B2 - - Google Patents
Info
- Publication number
- JPS6348806B2 JPS6348806B2 JP53046769A JP4676978A JPS6348806B2 JP S6348806 B2 JPS6348806 B2 JP S6348806B2 JP 53046769 A JP53046769 A JP 53046769A JP 4676978 A JP4676978 A JP 4676978A JP S6348806 B2 JPS6348806 B2 JP S6348806B2
- Authority
- JP
- Japan
- Prior art keywords
- molded body
- silicon
- graphite
- artificial graphite
- coated
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- 229910021383 artificial graphite Inorganic materials 0.000 claims description 16
- 229910052710 silicon Inorganic materials 0.000 claims description 15
- 239000010703 silicon Substances 0.000 claims description 15
- 239000011230 binding agent Substances 0.000 claims description 14
- 229910002804 graphite Inorganic materials 0.000 claims description 14
- 239000010439 graphite Substances 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 14
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 9
- 229910052726 zirconium Inorganic materials 0.000 claims description 9
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 8
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 8
- 239000010419 fine particle Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910026551 ZrC Inorganic materials 0.000 claims description 5
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 claims description 5
- 238000005260 corrosion Methods 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 239000011859 microparticle Substances 0.000 claims 2
- 239000010410 layer Substances 0.000 description 17
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 14
- 229920001568 phenolic resin Polymers 0.000 description 11
- 238000000034 method Methods 0.000 description 9
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 8
- 239000007788 liquid Substances 0.000 description 7
- 239000002002 slurry Substances 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 4
- 239000000945 filler Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000011247 coating layer Substances 0.000 description 3
- SLGWESQGEUXWJQ-UHFFFAOYSA-N formaldehyde;phenol Chemical compound O=C.OC1=CC=CC=C1 SLGWESQGEUXWJQ-UHFFFAOYSA-N 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229920003002 synthetic resin Polymers 0.000 description 2
- 239000000057 synthetic resin Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002006 petroleum coke Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/522—Graphite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/528—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components
- C04B35/532—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite obtained from carbonaceous particles with or without other non-organic components containing a carbonisable binder
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5053—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials non-oxide ceramics
- C04B41/5057—Carbides
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Products (AREA)
- Carbon And Carbon Compounds (AREA)
- Laminated Bodies (AREA)
Description
【発明の詳細な説明】
本発明は、結合剤を塗布されたグラフアイト
―、人造グラフアイト微粒子または人造グラフア
イトに類似の材料で造られた微粒子を用いて成形
され且つ腐蝕防止層を有する成形体を、未だ熱処
理に委ねていない生の成形体から出発して製造す
る方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention provides a molded product formed using graphite coated with a binder, artificial graphite fine particles, or fine particles made of a material similar to artificial graphite, and having a corrosion-inhibiting layer. The present invention relates to a method for producing a body starting from a green body which has not yet been subjected to heat treatment.
上記の種類の成形体の製造方法は公知である
(ドイツ特許第2040252号明細書参照)。例えば
かゝる成形体を製造する為の従来技術に属する一
つの方法は、最初に、フエノールホルムアルデヒ
ドの如き合成樹脂、ピツチ、タールまたはこれら
の類似物より成る結合剤が塗布されており且つ填
料として用いられる人造グラフアイトまたは人造
グラフアイトに類似の材料で造られているスラリ
ーから組成物を造るものである。グラフアイトと
しては石油コークス、電気グラフアイト、カーボ
ンブラツクまたはこれらの類似物の粉末が用いら
れる。この場合結合剤は、填料が懸濁された液体
中に完全にまたは一部分溶解される。次いでこの
溶液を、溶剤と混和し得てしかし結合剤を全く溶
解しないかまたは溶解し難い沈降処理用液中にい
れる。沈降処理用液としては例えば水が用いら
れ、結合剤としてフエノールホルムアルデヒドが
用いられる場合にはアルコールが用いられる。こ
の様にして形成されたスラリーを乾燥しそしてこ
うして得られる粉末を準備された成形用の型中に
入れ、次いで結合剤を完全にまたは部分的に溶解
している液体を蒸発させる。他の方法段階に於い
て成形体を乾燥しそして次いで粘結化する。 Methods for producing molded bodies of the above type are known (see German Patent No. 2040252). One method belonging to the prior art for producing such moldings, for example, is to first apply a binder consisting of a synthetic resin such as phenol formaldehyde, pitch, tar or the like and as a filler. The composition is made from a slurry made of the artificial graphite used or a material similar to the artificial graphite. As the graphite, petroleum coke, electrographite, carbon black or similar powders are used. In this case, the binder is completely or partially dissolved in the liquid in which the filler is suspended. This solution is then placed in a precipitation liquid that is miscible with the solvent but does not dissolve or dissolve the binder at all. For example, water is used as the settling liquid, and alcohol is used when phenol formaldehyde is used as the binder. The slurry thus formed is dried and the powder thus obtained is placed in a prepared mold, and the liquid in which the binder is completely or partially dissolved is then evaporated. In a further process step, the shaped body is dried and then caking.
フエノールホルムアルデヒド樹脂の如き合成樹
脂、ピツチまたはタールより成る結合剤が塗布さ
れ且つ填料として用いられる人造グラフアイトま
たは人造グラフアイトに類似の材料で形成された
スラリーから成形体を製造することも公知であ
る。この場合結合剤を、予め填料が懸濁されてい
る液体中に完全にまたは部分的に溶解し、次いで
その溶液を例えば水の如き、溶剤と混和し得手し
かし結合剤を全く溶解しないか溶解し難い液体中
に入れ、その上でその時に沈降するスラリーを取
り出す。このスラリーを最初乾燥し、その際に生
ずる粉末を準備された成形用の型に入れそして最
後に、結合剤を完全にまたは部分的に溶解してい
る液体を蒸発させる。この様にして造られる成形
体は次いで乾燥しそして粘結化する(ドイツ特許
第2133044号明細書参照)。 It is also known to produce molded bodies from slurries made of artificial graphite or materials similar to artificial graphite, coated with a binder consisting of a synthetic resin, such as a phenol formaldehyde resin, pitch or tar, and used as a filler. . In this case, the binder is completely or partially dissolved in the liquid in which the filler is previously suspended, and the solution is then miscible with a solvent, such as water, but does not dissolve the binder at all or dissolves it. It is placed in a difficult liquid, and then the slurry that settles out is taken out. This slurry is first dried, the resulting powder is placed in a prepared mold, and finally the liquid in which the binder is completely or partially dissolved is evaporated. The moldings produced in this way are then dried and caking (see German Patent No. 2,133,044).
成形体を製造する他の公知の一つの方法は、フ
エノールホルムアルデヒド樹脂で凝結した人造グ
ラフアイトまたは人造グラフアイトに類似の材料
を熱の供給下に100〜200℃の温度のもとで成形体
の表面から内部の方へ侵入するホルムアルデヒド
を用いてガス処理し、その際ガスの濃度が成形体
の予め決められた架橋度に依存しているものであ
る。 Another known method of producing a molded body is to form a molded body using artificial graphite or a material similar to artificial graphite precipitated with phenol formaldehyde resin at a temperature of 100 to 200°C under the supply of heat. Gas treatment is carried out using formaldehyde which penetrates from the surface into the interior, the concentration of the gas being dependent on the predetermined degree of crosslinking of the shaped body.
グラフアイトより成る成形体は、化学工業に於
いて反応を高温で実施することを必要とする場合
に、るつぼまたはその他の容器として広く用いら
れている。 Shaped bodies made of graphite are widely used as crucibles or other containers in the chemical industry where reactions need to be carried out at high temperatures.
しかしながら炭素材で造られた器具は、酸素の
影響下に用いたりまたは例えば反応の際に水蒸気
が形成される場合に腐蝕し易いという欠点を有し
ている。かゝる不利な結果を避ける為に、炭素ま
たはグラフアイトで製造されたるつぼまたはその
他の器具を保護するべき耐腐蝕性物質で被覆する
試みが既に行われて来た。これを達成しようとす
る公知の従来技術に属する一つの方法は、成形体
の腐蝕作用を受ける表面に被覆層をもたらすもの
である。公知のこの方法によれば、該被覆層は成
形体の表面で気相から炭化珪素または炭化ジルコ
ニウムを沈積することによつて形成される。他の
公知の方法では、プラズマを用いて炭化珪素また
は炭化ジルコニウムを液化しそして反応容器また
は―器具の保護すべき表面に吹きつけるものであ
る。しかしこの公知の方法には、非常に費用が
かゝるという欠点がある。更に重大な欠点は、こ
の様に造られた層が、即ちるつぼまたはその他の
器具の材料として用いられた炭素またはグラフア
イトと形成された層の炭化珪素または炭化ジルコ
ニウムと異なる熱膨脹係数を有していることであ
る。例えば、一般に用いられる炭素材料の熱膨脹
係数は室温のもとで1・10-5〜1・10-6の大きさ
であり、一方SiCのそれは6.6・10-6である。かゝ
る異なつた挙動が、SiC―層を既に塗布後の冷却
の際に度々破裂させてしまい、それ故に器具が所
定の用途に於いて非常に僅かの寿命しか有さない
という不利な原因に成つている。 However, devices made of carbon materials have the disadvantage that they are susceptible to corrosion when used under the influence of oxygen or when, for example, water vapor is formed during the reaction. In order to avoid such adverse consequences, attempts have already been made to coat crucibles or other instruments made of carbon or graphite with protective corrosion-resistant materials. One method known in the prior art for achieving this is to provide a coating layer on the corrosive surface of the molded body. According to this known method, the coating layer is formed by depositing silicon carbide or zirconium carbide from the gas phase on the surface of the molded body. Another known method uses a plasma to liquefy silicon carbide or zirconium carbide and spray it onto the surface of the reaction vessel or equipment to be protected. However, this known method has the disadvantage that it is very expensive. A further serious drawback is that the layer thus produced has a different coefficient of thermal expansion than the silicon carbide or zirconium carbide layer formed with the carbon or graphite used as material for the crucible or other device. It is that you are. For example, the coefficient of thermal expansion of commonly used carbon materials is on the order of 1.10 -5 to 1.10 -6 at room temperature, while that of SiC is 6.6.10 -6 . Such a different behavior has the disadvantage that the SiC layer often ruptures even during cooling after application and therefore the device has a very short service life in a given application. It is completed.
本発明の課題は、高い負荷のもとでも長い寿命
を有する塗布層を持つた、グラフアイト、人造グ
ラフアイトまたは人造グラフアイトに類似の材料
より成る成形体の製造方法を見出すことにある。
更にこの方法は大きな成形体を造る為にも用いる
ことができるべきである。 The object of the invention is to find a method for producing molded bodies made of graphite, artificial graphite or materials similar to artificial graphite, which have a coating layer that has a long service life even under high loads.
Furthermore, the method should also be able to be used for producing large molded bodies.
この課題は、初めに述べた種類の成形体に、内
側の層から外側の層へ0原子%から(即ち、成形
体から)50原子%まで増加する珪素―またはジル
コニウム含有量で珪素またはジルコニウムが混入
された上記成形体の材質より成る2種類以上の層
を被覆することによつて解決される。 The task is to apply silicon or zirconium to a shaped body of the type mentioned at the outset with a silicon- or zirconium content increasing from 0 at. % to 50 at. % (i.e. from the shaped body) from the inner layer to the outer layer. This problem can be solved by coating with two or more types of layers made of the mixed materials of the molded body.
こうして被覆される成形体は非常に簡単に製造
できる。本発明では、結合剤を塗布したグラフア
イト―、人造グラフアイト微粒子または人造グラ
フアイトに類似の材料で造られた微粒子から成形
された成形体を最初に製造し、これに続いて、0
原子%から(即ち、成形体から)50原子%まで珪
素またはジルコニウムを混入した前記成形体用の
材料より成る多種類の組成物の被覆物を成形体に
層状に、しかも中心に近い層は珪素―またはジル
コニウム含有量が最も少なくそして外側層は珪素
―またはジルコニウム含有量が最も多いように塗
布し、その上でこうして被覆された成形体を保護
ガス雰囲気下に650〜850℃の間の温度のもとで粘
結化しそしてこれに続いて、外側層に炭化珪素ま
たは炭化ジルコニウムを形成する為に、速い加熱
速度で約1550℃〜1800℃の温度にする。この方法
で製造される成形体は負荷および寿命に関して所
期の要求を全く満足するものである。 Molded bodies coated in this way can be produced very simply. In the present invention, a molded body is first produced from graphite coated with a binder, artificial graphite fine particles, or fine particles made of a material similar to artificial graphite, and then
The molded body is coated with coatings of various compositions of the above-mentioned molded body material containing from atomic % to 50 atomic % (i.e. from the molded body) of silicon or zirconium, with the layer near the center containing silicon or zirconium. - or the lowest zirconium content and the outer layer is silicon - or the highest zirconium content, and the molded body thus coated is then heated under a protective gas atmosphere at a temperature between 650 and 850°C. Temperatures of about 1550 DEG C. to 1800 DEG C. are reached at a rapid heating rate in order to caking and subsequent formation of silicon carbide or zirconium carbide in the outer layer. The molded bodies produced in this way fully meet the desired requirements with regard to load and service life.
実施例
最初に、結合材としてフエノールホルムアルデ
ヒド樹脂およびこのものを塗布された電気グラフ
アイト微粒子より成る組成物を造りそしてこのも
のから成形体を製造する。これに関連して、成形
体を製造する為に用いた組成物に、フエノールホ
ルムアルデヒドで被覆した珪素粉末を添加混合す
る。その際に種々の珪素含有量の組成物を造る。
即ち、以下の組成物である:
組成物1:(Si:C=0.2:1)
珪素量 278.4g
フエノールホルムアルデヒド樹脂量 250.0g
グラフアイト量 471.6g
組成物2:(Si:C=0.4:1)
珪素量 422.4g
フエノールホルムアルデヒド樹脂量 250.0g
グラフアイト量 327.6g
組成物3:(Si:C=0.6:1)
珪素量 510.4g
フエノールホルムアルデヒド樹脂量 250.0g
グラフアイト量 239.6g
組成物4:(Si:C=0.8:1)
珪素量 569.8g
フエノールホルムアルデヒド樹脂量 250.0g
グラフアイト量 180.2g
組成物5:(Si:C=1:1)
珪素量 612.5g
フエノールホルムアルデヒド樹脂量 250.0g
グラフアイト量 137.5g
これらの組成物を約1〜2mmの厚さの層として
順次に成形体に塗布し、その際成形体に隣接する
層は最も少ない珪素含有量を示し(要するに、最
初の組成物で造られている)そして外側に向かつ
てこれに続くそれぞれの層は段階的に多い珪素含
有量を示しそして外側の層は最も大きい珪素含有
量を示す(要するに、組成物5で造られている)。
次いでこうして被覆された成形体を、粘結化する
為に800℃の温度にまで加熱する。その上で被覆
されたこの成形体を約30℃/分の加熱速度で1800
℃の温度に加熱す、次いで冷却する。上記温度に
加熱した為に外側面に炭化珪素層が形成されたこ
とが判つた。この層は高い負荷のもとでも大きな
付着強度を示しそして所望の耐腐蝕性を有してい
る。EXAMPLE First, a composition consisting of a phenol formaldehyde resin as a binder and electrographite fine particles coated with this is prepared, and a molded body is produced from this. In this connection, silicon powder coated with phenol formaldehyde is added and mixed into the composition used for producing the molded body. In this case, compositions with different silicon contents are produced.
That is, the composition is as follows: Composition 1: (Si:C=0.2:1) Silicon amount 278.4g Phenol formaldehyde resin amount 250.0g Graphite amount 471.6g Composition 2: (Si:C=0.4:1) Amount of silicon 422.4g Amount of phenol formaldehyde resin 250.0g Amount of graphite 327.6g Composition 3: (Si:C=0.6:1) Amount of silicon 510.4g Amount of phenol formaldehyde resin 250.0g Amount of graphite 239.6g Composition 4: (Si: C=0.8:1) Amount of silicon 569.8g Amount of phenol formaldehyde resin 250.0g Amount of graphite 180.2g Composition 5: (Si:C=1:1) Amount of silicon 612.5g Amount of phenol formaldehyde resin 250.0g Amount of graphite 137.5g are applied to the shaped body in successive layers of a thickness of approximately 1 to 2 mm, with the layer adjacent to the shaped body having the lowest silicon content (in short, the layers made of the first composition ) and each successive layer towards the outside exhibits a progressively higher silicon content, with the outer layer exhibiting the highest silicon content (in short, made with composition 5).
The molded body thus coated is then heated to a temperature of 800° C. for caking. The coated molded body was heated to 1800°C at a heating rate of approximately 30°C/min.
heating to a temperature of °C, then cooling. It was found that a silicon carbide layer was formed on the outer surface due to heating to the above temperature. This layer exhibits high adhesive strength even under high loads and has the desired corrosion resistance.
Claims (1)
フアイト微粒子または人造グラフアイトに類似の
材料で造られた微粒子から成形された成形体を最
初に製造し、これに続いて、0原子%から(即
ち、成形体から)50原子%まで珪素またはジルコ
ニウムを混入した前記成形体用の材料より成る多
種類の組成物の被覆物を成形体に層状に、しかも
中心に近い層は珪素―またはジルコニウム含有量
が最も少なくそして外側層は珪素―またはジルコ
ニウム含有量が最も多いように塗布し、その上で
こうして被覆された成形体を保護ガス雰囲気下に
650〜850℃の間の温度のもとで粘結化しそしてこ
れに続いて、外側層に炭化珪素または炭化ジルコ
ニウムを形成する為に、速い加熱速度で約1550℃
〜1800℃の温度にすることを特徴とする、結合剤
を塗布したグラフアイト―、人造グラフアイト微
粒子または人造グラフアイトに類似の材料から造
られた微粒子を用いて成形され且つ腐蝕防止層を
有する成形体であつて、成形体が内側の層から外
側の層へ0原子%から(即ち、成形体から)50原
子%へ増加する珪素―またはジルコニウム含有量
で珪素またはジルコニウムを混入した成形体の材
質より成る多種類の層によつて被覆されている上
記成形体の製造方法。1. A molded body formed from binder-coated graphite, artificial graphite microparticles or microparticles made of a material similar to artificial graphite is first produced, and this is followed by , from the molded body) are layered on the molded body with coatings of various compositions of the above-mentioned molded body materials containing up to 50 at. and the outer layer is applied with the highest silicon or zirconium content, and the thus coated molded body is then placed under a protective gas atmosphere.
About 1550°C at a fast heating rate to caking under temperatures between 650 and 850°C and following this to form silicon carbide or zirconium carbide in the outer layer.
Shaped using graphite coated with a binder, artificial graphite fine particles or fine particles made from a material similar to artificial graphite, characterized by a temperature of ~1800°C, and having an anti-corrosion layer A shaped body, the shaped body being doped with silicon or zirconium, with a silicon- or zirconium content increasing from 0 at. % to 50 at. % (i.e. from the shaped body) from the inner layer to the outer layer. A method for producing the above-mentioned molded article, which is covered with various layers made of different materials.
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19772718143 DE2718143C3 (en) | 1977-04-23 | 1977-04-23 | Process for the production of shaped bodies formed from graphite or from a graphite-like material with a protective layer made of carbide |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS53133208A JPS53133208A (en) | 1978-11-20 |
JPS6348806B2 true JPS6348806B2 (en) | 1988-09-30 |
Family
ID=6007098
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP4676978A Granted JPS53133208A (en) | 1977-04-23 | 1978-04-21 | Moldings formed with particulates made of graphite artificial graphite particulates or materials similar to artificial graphite and having antii corrosion layer* and production thereof |
Country Status (3)
Country | Link |
---|---|
JP (1) | JPS53133208A (en) |
DE (1) | DE2718143C3 (en) |
FR (1) | FR2387922A1 (en) |
Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3005587A1 (en) * | 1980-02-15 | 1981-08-20 | Kernforschungsanlage Jülich GmbH, 5170 Jülich | METHOD FOR PRODUCING MOLDED BODIES |
US4702960A (en) * | 1980-07-30 | 1987-10-27 | Avco Corporation | Surface treatment for carbon and product |
US4340636A (en) * | 1980-07-30 | 1982-07-20 | Avco Corporation | Coated stoichiometric silicon carbide |
DE102006040309B4 (en) | 2006-08-29 | 2009-04-16 | Ald Vacuum Technologies Gmbh | Spherical fuel assembly and its manufacture for gas-cooled high-temperature ball-puffed nuclear reactors (HTR) |
DE102007056135A1 (en) * | 2007-11-20 | 2009-05-28 | Ald Vacuum Technologies Gmbh | Reactor graphite consisting of isotropic highly crystalline natural graphite as the main component and silicon or zirconium carbide and its preparation |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5346770A (en) * | 1976-10-12 | 1978-04-26 | Citizen Watch Co Ltd | Winding stem mounting and dismounting structure of wristwatches |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2040252C3 (en) | 1970-08-13 | 1974-05-30 | Kernforschungsanlage Juelich Gmbh, 5170 Juelich | Process for the production of artificial graphite and graphite-like materials |
DE2133044C3 (en) | 1971-07-02 | 1975-10-02 | Kernforschungsanlage Juelich Gmbh, 5170 Juelich | Process for the production of shaped bodies from synthetic graphite or materials similar to synthetic graphite |
-
1977
- 1977-04-23 DE DE19772718143 patent/DE2718143C3/en not_active Expired
-
1978
- 1978-04-19 FR FR7811534A patent/FR2387922A1/en active Granted
- 1978-04-21 JP JP4676978A patent/JPS53133208A/en active Granted
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5346770A (en) * | 1976-10-12 | 1978-04-26 | Citizen Watch Co Ltd | Winding stem mounting and dismounting structure of wristwatches |
Also Published As
Publication number | Publication date |
---|---|
DE2718143A1 (en) | 1978-11-16 |
DE2718143C3 (en) | 1979-10-31 |
FR2387922A1 (en) | 1978-11-17 |
DE2718143B2 (en) | 1979-03-08 |
JPS53133208A (en) | 1978-11-20 |
FR2387922B1 (en) | 1984-01-27 |
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